US9281465B2 - Piezoelectric element and method of manufacturing the same - Google Patents

Piezoelectric element and method of manufacturing the same Download PDF

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US9281465B2
US9281465B2 US13/903,737 US201313903737A US9281465B2 US 9281465 B2 US9281465 B2 US 9281465B2 US 201313903737 A US201313903737 A US 201313903737A US 9281465 B2 US9281465 B2 US 9281465B2
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piezoelectric
manganese
internal electrodes
piezoelectric element
piezoelectric ceramic
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US20140028156A1 (en
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Hiroyuki Shimizu
Keiichi Hatano
Yutaka Doshida
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Taiyo Yuden Co Ltd
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N30/00—Piezoelectric or electrostrictive devices
    • H10N30/80—Constructional details
    • H10N30/85—Piezoelectric or electrostrictive active materials
    • H10N30/853—Ceramic compositions
    • H01L41/187—
    • H01L41/1873—
    • H01L41/273—
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N30/00—Piezoelectric or electrostrictive devices
    • H10N30/01—Manufacture or treatment
    • H10N30/05—Manufacture of multilayered piezoelectric or electrostrictive devices, or parts thereof, e.g. by stacking piezoelectric bodies and electrodes
    • H10N30/053—Manufacture of multilayered piezoelectric or electrostrictive devices, or parts thereof, e.g. by stacking piezoelectric bodies and electrodes by integrally sintering piezoelectric or electrostrictive bodies and electrodes
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N30/00—Piezoelectric or electrostrictive devices
    • H10N30/80—Constructional details
    • H10N30/85—Piezoelectric or electrostrictive active materials
    • H10N30/853—Ceramic compositions
    • H10N30/8542—Alkali metal based oxides, e.g. lithium, sodium or potassium niobates

Definitions

  • the present invention relates to a piezoelectric element containing Pb-free piezoelectric ceramics, as well as a manufacturing method thereof.
  • Piezoelectric ceramics are used as piezoelectric elements. Piezoelectric elements are used as sensor elements, generation elements, and the like, by applying the piezoelectric effect of converting mechanical energy to electrical energy. Piezoelectric elements are also used as vibrators, sound generators, actuators, ultrasonic motors, etc., that apply the reverse-piezoelectric effect of converting electrical energy to mechanical energy. In addition, piezoelectric elements are used as circuit elements, vibration control elements, etc., by combining the piezoelectric effect and reverse-piezoelectric effect.
  • a piezoelectric element has a structure comprising layered piezoelectric ceramic sheets and internal electrodes placed between the layers.
  • a piezoelectric element has two terminals and its internal electrodes are connected alternately to the different terminals. This way, voltage is applied to each piezoelectric ceramic layer when voltage is applied between the terminals.
  • PZT material expressed by the composition formula Pb(Zr,Ti)O 3 —PbTiO 3 and PLZT material expressed by the composition formula (Pb,La)(Zr,Ti)O 3 —PbTiO 3 , are widely known.
  • piezoelectric ceramics having a perovskite structure of alkali-containing niobate (refer to Patent Literatures 1 to 7 and Non-patent Literatures 1 and 2) or of barium titanate (refer to Patent Literature 8) are known as offering relatively good performance.
  • Patent Literature 7 discloses a piezoelectric ceramic offering improved piezoelectric characteristics, achieved by dispersing a sub phase containing the composition K 3 Nb 3 O 6 Si 2 O 7 in the main phase of alkali-containing niobate perovskite structure and thereby producing a dense structure constituted by grains of uniform size.
  • Patent Literature 1 Japanese Patent Laid-open No. 2002-068825
  • Patent Literature 2 Japanese Patent Laid-open No. 2003-342069
  • Patent Literature 3 Japanese Patent Laid-open No. 2004-300012
  • Patent Literature 4 Japanese Patent Laid-open No. 2008-207999
  • Patent Literature 5 International Patent Laid-open No. 2008/152851
  • Patent Literature 6 Japanese Patent Laid-open No. 2010-180121
  • Patent Literature 7 Japanese Patent Laid-open No. 2010-052999
  • Patent Literature 8 Japanese Patent Laid-open No. 2002-208743
  • Non-patent Literature 1 Nature, 432 (4), 2004, pp. 84-87
  • Piezoelectric elements are required to have high insulation characteristics between their internal electrodes, or specifically high insulation characteristics of their piezoelectric ceramic layers.
  • the piezoelectric ceramic disclosed in Cited Literature 7 has a fine structure and consequently many grain boundaries in the direction in which voltage is applied. Since piezoelectric ceramics generally have higher insulation property at the grain boundaries than inside the crystal grains, the aforementioned piezoelectric ceramic provides good insulation characteristics desired of piezoelectric ceramic layers constituting piezoelectric elements.
  • piezoelectric elements are subject to a drop in insulation characteristics if any one of their piezoelectric layers undergoes dielectric breakdown as a result of deterioration of the piezoelectric ceramic layer occurring over the course of use.
  • an object of the present invention is to provide a piezoelectric element whose insulation performance is kept from dropping over the course of use, as well as a manufacturing method of such piezoelectric element.
  • a piezoelectric element pertaining to an embodiment of the present invention comprises first internal electrodes and second internal electrodes, as well as piezoelectric ceramic layers that are made of ceramic and arranged between the first internal electrodes and second internal electrodes.
  • Manganese is present relatively more abundantly in the areas of the piezoelectric ceramic layers adjacent to the first internal electrodes and second internal electrodes, compared to at the centers of the piezoelectric ceramic layers.
  • a manufacturing method of piezoelectric element pertaining to an embodiment of the present invention comprises: forming ceramic sheets containing manganese element; dispersing crystal containing manganese element on both sides of the ceramic sheets; applying an electrode paste to the ceramic sheets on which the crystal containing manganese element has been dispersed, to form electrodes; laminating the ceramic sheets having the electrodes formed on them, to form a laminate; and sintering the laminate.
  • FIG. 1 is a schematic diagram of the unit lattice of a perovskite structure.
  • FIG. 2A is a perspective view of a piezoelectric element pertaining to an embodiment of the present invention.
  • FIG. 2B is a section view of the piezoelectric element shown in FIG. 2A , cut along line A-A′.
  • FIG. 3 is a flow chart indicating the manufacturing method of the piezoelectric element shown in FIG. 2A .
  • FIG. 4A is a schematic drawing illustrating the manganese dispersion step performed to make the piezoelectric element shown in FIG. 2A .
  • FIG. 4B is a schematic drawing illustrating the manganese dispersion step performed to make the piezoelectric element shown in FIG. 2A .
  • FIG. 5A is a schematic drawing illustrating the internal electrode paste application step performed to make the piezoelectric element shown in FIG. 2A .
  • FIG. 5B is a schematic drawing illustrating the internal electrode paste application step performed to make the piezoelectric element shown in FIG. 2A .
  • FIG. 6 is a schematic drawing illustrating the ceramic sheet lamination step performed to make the piezoelectric element shown in FIG. 2A .
  • FIG. 7A is a schematic drawing illustrating the external electrode forming step performed to make the piezoelectric element shown in FIG. 2A .
  • FIG. 7B is a schematic drawing illustrating the external electrode forming step performed to make the piezoelectric element shown in FIG. 2A .
  • FIG. 9A is a graph showing how the piezoelectric constant d 33 changes relative to the content of Mn.
  • FIG. 9B is a graph showing how the DC insulation longevity changes relative to the content of Mn.
  • FIG. 9C is a graph showing how the AC insulation longevity changes relative to the content of Mn.
  • a piezoelectric element pertaining to an embodiment of the present invention comprises first internal electrodes and second internal electrodes, as well as piezoelectric ceramic layers that are made of ceramics and arranged between the first internal electrodes and second internal electrodes.
  • Manganese is present relatively more abundantly in the areas of the piezoelectric ceramic layers adjacent to the first internal electrodes and second internal electrodes, compared to at the centers of the piezoelectric ceramic layers. With a piezoelectric element of this structure, its insulation performance is kept from dropping over the course of use.
  • the aforementioned areas may extend over the entire surfaces of the first electrodes and second electrodes.
  • Manganese may be present at the grain boundaries of the ceramics, especially at crystal grain triple points. With a piezoelectric element of this structure, its insulation performance is kept from dropping over the course of use without the piezoelectric effect being obstructed in any way.
  • the piezoelectric ceramic layers may have crystals containing manganese as mentioned above.
  • the piezoelectric ceramic layers may also have crystals containing manganese unevenly distributed over the aforementioned areas. Additionally, the crystals containing manganese may be crystals whose mother phase is MnO. Moreover, the crystals containing manganese in the piezoelectric ceramic layers may have an average grain size of 0.1 ⁇ m or more but 5 ⁇ m or less. With a piezoelectric element of this structure, its insulation performance is kept from dropping over the course of use without the piezoelectric effect being obstructed in any way.
  • the piezoelectric element may also have a first external electrode and second external electrode, with the first internal electrodes and second internal electrodes placed alternately via the piezoelectric ceramic layers and the first internal electrodes each connected to the first external electrode, while the second internal electrodes each connected to the second external electrode.
  • a piezoelectric element of this structure offers excellent piezoelectric characteristics because it has a so-called layered structure.
  • the piezoelectric ceramic layers may have a thickness of 10 ⁇ m or more but 60 ⁇ m or less.
  • the piezoelectric ceramic layers may have an alkali-containing niobate perovskite structure as its main phase.
  • the main phase may be one expressed by the composition formula (Li x Na y K 1-x-y ) a (Nb 1-z Ta z )O 3 (in the formula, 0.04 ⁇ x ⁇ 0.1, 0 ⁇ y ⁇ 1, 0 ⁇ z ⁇ 0.4, 0.95 ⁇ a ⁇ 1.01, and x+y ⁇ 1).
  • a piezoelectric element of this structure excellent piezoelectric characteristics can be achieved because a piezoelectric composition of high piezoelectric characteristics is used as its main phase.
  • the piezoelectric ceramic layers contain manganese at a ratio of 0.2 mol or more but 2.0 mol or less relative to 100 mol of the main phase.
  • a piezoelectric element of this structure offers excellent insulation property due to the action of the phase containing manganese in the piezoelectric ceramic layers.
  • the piezoelectric ceramic layers may contain silicon at a ratio of 0.2 mol or more but 3.0 mol or less relative to 100 mol of the main phase.
  • a piezoelectric element of this structure offers excellent insulation performance and mechanical strength because the piezoelectric ceramic layers have a dense and uniform structure.
  • a manufacturing method of a piezoelectric element pertaining to an embodiment of the present invention comprises: forming ceramic sheets containing manganese; dispersing crystals containing manganese on both sides of the ceramic sheets; applying an electrode paste to the ceramic sheets on which the crystals containing manganese have been dispersed, to form electrodes; laminating the ceramic sheets having the electrodes formed on them, to form a laminate; and sintering the laminate.
  • the piezoelectric ceramic pertaining to this embodiment, a piezoelectric ceramic whose main phase comprises an alkali-containing niobate perovskite structure was used.
  • the piezoelectric ceramic is constituted by a polycrystalline expressed by Composition Formula (1) below: (Li x Na y K 1-x-y ) a (Nb 1-z Ta z )O 3 (1)
  • FIG. 1 is a model of the unit lattice of a perovskite structure.
  • a perovskite structure is expressed by the composition formula ABO 3 , comprising the atoms conformationally positioned at site A, atoms conformationally positioned at site B, and oxygen (O) atoms.
  • ABO 3 composition formula
  • oxygen (O) atoms As shown in FIG. 1 , in a perovskite structure six oxygen atoms are arranged around the atoms at site B, 12 oxygen atoms are arranged around the atoms at site A, and these structures are repeated cyclically to form crystals.
  • Li, Na, and K are conformationally positioned at site A in FIG. 1
  • Nb and Ta are conformationally positioned at site B.
  • the elements conformationally positioned at site A, or specifically Li, Na, and K are prone to deficiency due to volatilization during sintering, etc., and specifically they may decrease by around several percent to two percent from the level in the stoichiometric composition. Accordingly, it is possible to obtain a stable perovskite structure close to the stoichiometric composition by predicting the deficiencies in Li, Na, and K and increasing Li, Na, and K accordingly from the levels in the stoichiometric composition in the initial composition (composition when weighed). To be specific, it is known that a stable perovskite structure can be obtained when the range of a in Composition Formula (1) is 0.95 ⁇ a ⁇ 1.01.
  • the piezoelectric ceramic pertaining to this embodiment may be constituted in such a way that a sub phase is dispersed in the main phase.
  • the sub phase include a manganese-containing phase, silicon-containing phase, lithium-containing phase, alkali-earth-metal-containing phase and zirconium-containing phase, among others.
  • Insulation characteristics of piezoelectric ceramics can be improved by dispersing a manganese-containing phase as a sub phase.
  • the manganese-containing phase itself does not contribute to piezoelectric characteristics, which means that piezoelectric characteristics of piezoelectric ceramics will drop if the manganese-containing phase, which is a sub phase, is excessive relative to the main phase.
  • a manganese-containing phase is intentionally distributed unevenly inside the piezoelectric ceramic to improve the insulation performance of the piezoelectric element while maintaining its piezoelectric characteristics.
  • the manganese-containing phase which is primarily present in a state of MnO, may also be present in a state of MnO 2 or Mn 3 O 4 .
  • the manganese-containing phase need not constitute crystals, but it can also be present as an amorphous phase.
  • a piezoelectric ceramic having a main phase of uniform fine crystal structure can be obtained by dispersing a silicon-containing phase as a sub phase.
  • the finer the crystals of the piezoelectric ceramic the higher the quantity of the grain boundaries found in the unit volume of piezoelectric ceramic become. As a result, the insulation characteristics of the piezoelectric ceramic will improve, and so will its mechanical strength.
  • the silicon-containing phase itself does not contribute to piezoelectric characteristics, which means that piezoelectric characteristics of a piezoelectric ceramic will drop if the silicon-containing phase, which is a sub phase, is excessive relative to the main phase. It is known that a favorable content of silicon-containing phase is 0.2 mol or more but 3.0 mol or less of silicon relative to 100 mol of the main phase.
  • the silicon-containing phase may be present in a state of SiO 2 , but preferably it is present in a state of K 3 Nb 3 O 6 Si 2 O 7 .
  • a method can be adopted whereby a K 3 Nb 3 O 6 Si 2 O 7 powder is prepared separately from the powder of main phase and a mixed powder comprising this powder and powder of the main phase is sintered.
  • Another method that can be adopted is to separate K 3 Nb 3 O 6 Si 2 O 7 when a mixed powder comprising the powder of main phase and SiO 2 powder is sintered.
  • sintering property of piezoelectric ceramic can be improved by using Li 2 O or Li 2 CO 3 as a sintering auxiliary when the piezoelectric ceramic is sintered. This is specifically because the Li contained in Li 2 O or Li 2 CO 3 acts in a manner compensating for the deficiencies in the elements at site A during sintering.
  • a lithium-containing phase may remain in the sintered piezoelectric ceramic as a sub phase.
  • the lithium-containing phase may be present in a state of Li 2 O, for example.
  • Li 2 O or Li 2 CO 3 used as a sintering auxiliary will improve the sintering property of piezoelectric ceramic without having any negative impact on the characteristics of piezoelectric ceramic as long as its content is 0.1 mol or more but 1.5 mol or less relative to 100 mol of the main phase.
  • sintering property of piezoelectric ceramic can be improved by using an oxide containing alkali earth metal, as a sintering auxiliary, when the piezoelectric ceramic is sintered.
  • the alkali earth metal contained in this oxide acts in a manner compensating for the deficiencies in the elements at site A, while also compensating for the decreases in valences at site A.
  • at least one of Ca, Ba, and Sr can be adopted for this alkali earth metal.
  • a zirconium-containing oxide can be added to the piezoelectric ceramic pertaining to this embodiment for the purpose of preventing its insulation property from dropping.
  • zirconium-containing oxide include ZrO 2 , among others.
  • a composition containing at least one of Sc, Ti, V, Cr, Fe, Co, Cu, and Zn, all of which are first transition elements, can be added to the piezoelectric ceramic pertaining to this embodiment, for example, for the purpose of controlling the sintering temperature and suppressing the growth of crystal grains.
  • a composition containing at least one of Y, Mo, Ru, Rh and Pd, all of which are second transition elements, can be added to the piezoelectric ceramics pertaining to this embodiment, for example, for the purpose of controlling the sintering temperature, suppressing the growth of crystal grains and extending the longevity in a high electric field.
  • a composition containing at least one of La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Hf, W, Re, Os, Ir, Pt, and Au, all of which are third transition elements, can be added to the piezoelectric ceramics pertaining to this embodiment, for example, for the purpose of controlling the sintering temperature, suppressing the growth of crystal grains, and extending the longevity in a high electric field.
  • a complex composition comprising transition elements selected from the aforementioned first transition elements, second transition elements, and third transition elements can also be added to the piezoelectric ceramic pertaining to this embodiment.
  • FIGS. 2A and 2B show the piezoelectric element 10 pertaining to this embodiment, where FIG. 2A is a perspective view, while FIG. 2B is a section view of FIG. 2A , cut along line A-A′.
  • the piezoelectric element 10 is constituted by a piezoelectric ceramic 11 and external electrodes 14 , 15 provided at both ends in the Y-axis direction of the piezoelectric ceramic 11 .
  • the piezoelectric element 10 also has two types of internal electrodes 12 , 13 that extend in the directions along the XY plane inside the piezoelectric ceramic 11 and are arranged alternately in a manner opposing each other in the Z-axis direction.
  • the number of internal electrodes 12 , 13 can be determined arbitrarily. All of the internal electrodes 12 are connected to the external electrode 14 , while all of the internal electrodes 13 are connected to the external electrode 15 .
  • the thickness of internal electrodes 12 , 13 in the Z-axis direction can be determined as deemed appropriate. For example, the thickness of internal electrodes 12 , 13 in the Z-axis direction may be 0.5 ⁇ m or more but 2 ⁇ m or less.
  • FIG. 2B shows, as a matter of convenience for illustration purposes, an example where six piezoelectric ceramic 11 layers are arranged between the internal electrodes 12 , 13 , but the number of piezoelectric ceramic 11 layers can be determined arbitrarily according to the purpose, etc. In other words, there can be any number of piezoelectric ceramic 11 layers as long as there is one or greater.
  • the top layer and bottom layer in the Z-axis direction which are not arranged between the internal electrodes 12 , 13 , do not achieve any piezoelectric effect when the piezoelectric element 10 is used. Accordingly, the top layer and bottom layer of the piezoelectric element 10 in the Z-axis direction need not be constituted by the piezoelectric ceramic 11 . Still, preferably the top layer and bottom layer of the piezoelectric element 10 in the Z-axis direction are constituted by insulation material in order to prevent electrical continuity between the external electrodes 14 , 15 .
  • the internal electrodes 12 , 13 of the piezoelectric element 10 are constituted as Pt electrodes which are conductive layers containing Pt as their main constituent. However, the internal electrodes 12 , 13 need not be Pt electrodes, but they can also be Pd electrodes or Ag—Pd electrodes, for example.
  • the external electrodes 14 , 15 of the piezoelectric element 10 are constituted as Ag electrodes which are conductors whose main constituent is Ag. However, the external electrodes 14 , 15 need not be Ag electrodes, but they can also be constituted by Pb-free solder, for example.
  • applying voltage between the external electrodes 14 , 15 has the effect of applying voltage between the internal electrodes 12 , 13 that are adjacent to each other.
  • Each piezoelectric ceramic 11 layer between the internal electrodes 12 , 13 exhibits a varying degree of piezoelectric effect according to the voltage applied between the internal electrodes 12 , 13 , and deforms by expanding or contracting in the Z-axis direction.
  • areas adjacent to the internal electrodes 12 , 13 in the Z-axis direction contain a manganese-rich phase 11 b (these areas are specifically where there is an abundance of manganese in the piezoelectric ceramic phase 11 , or, in other words, areas to which manganese is unevenly distributed).
  • the areas adjacent to the internal electrodes 12 , 13 in the Z-axis direction include the surfaces of piezoelectric ceramic 11 contacting the internal electrodes 12 , 13 and extend in the directions along the XY plane.
  • the areas adjacent to the internal electrodes 12 , 13 in the Z-axis direction have a certain depth in the Z-axis direction from the surfaces of piezoelectric ceramic 11 contacting the internal electrodes 12 , 13 toward the center of the piezoelectric ceramic 11 .
  • the depth in the Z-axis direction of the areas adjacent to the internal electrodes 12 , 13 in the Z-axis direction may be one-third the thickness of the piezoelectric ceramic 11 , for example.
  • the manganese-rich phase 11 b is constituted by the main phase of the piezoelectric ceramic phase 11 in which a manganese-containing phase that contains manganese is dispersed. Accordingly, in the manganese-rich phase 11 b a manganese-containing phase offering high insulation property is dispersed in the directions along the XY plane. In other words, in the piezoelectric element 10 a manganese-rich phase 11 b is formed in each piezoelectric ceramic 11 layer to intentionally and unevenly distribute manganese in the areas adjacent to the internal electrodes 12 , 13 .
  • the manganese-rich phase 11 b not only enhances the insulation property between the internal electrodes 12 , 13 , but it also functions to disperse the electric field applied to the piezoelectric ceramic phase 11 from the internal electrodes 12 , 13 . This prevents the electric field from concentrating locally in each piezoelectric ceramic 11 layer of the piezoelectric element 10 , thereby making each piezoelectric ceramic 11 layer resistant to dielectric breakdown and consequently to insulation failure.
  • the piezoelectric element 10 may be constituted in such a way that manganese is present relatively more abundantly in the areas of piezoelectric ceramic 11 adjacent to the first internal electrodes 12 and second internal electrodes 13 , respectively, compared to at the centers of piezoelectric ceramic 11 , in order to enhance the aforementioned effects.
  • each piezoelectric ceramic 11 layer does not diminish its piezoelectric characteristics, at least in the areas other than the manganese-rich phase 11 b , due to the presence of manganese. Accordingly, with the piezoelectric element 10 a manganese-rich phase 11 b is intentionally formed to keep its insulation performance from dropping over the course of use without sacrificing its piezoelectric characteristics in any way.
  • a manganese-rich phase 11 b is formed in both of the areas adjacent to the internal electrodes 12 , 13 in the Z-axis direction.
  • the purpose of the art of the present invention can be achieved as long as a manganese-rich phase 11 b is formed in at least one of the areas adjacent to the internal electrodes 12 , 13 .
  • examples of the manganese-containing phase in the manganese-rich phase 11 b include oxides whose mother phase is manganese monoxide (MnO), manganese dioxide (MnO 2 ), or trimanganese tetraoxide (Mn 3 O 4 ), among others.
  • the manganese-containing phase need not be an oxide whose mother phase is an oxide containing manganese only, but it can also be an oxide whose mother phase is an oxide constituted by a complete solid solution of manganese and other metal, for example. Additionally, the manganese-containing phase need not be constituted by crystals, but it can also be an amorphous phase.
  • the average grain size of the manganese-containing oxide crystals in the manganese-rich phase 11 b is 0.1 ⁇ m or more but 5 ⁇ m or less. If the average grain size of the manganese-containing oxide crystals exceeds 5 ⁇ m, electric field response in the main phase may deteriorate and piezoelectric characteristics may drop. If the average grain size of the manganese-containing oxide crystals is less than 0.1 ⁇ m, on the other hand, the aforementioned drop in insulation performance cannot be suppressed effectively.
  • the crystal grain size was calculated as the so-called area-equivalent size.
  • a section of the crystal structure was observed by a SEM (scanning electron microscope) and a circle diameter resulting in an area equivalent to the area of a crystal grain was used as the size of the crystal grain.
  • the average grain size of crystals can be obtained as an average size of crystal grains present in a 100 ⁇ m ⁇ 100 ⁇ m area of the crystal structure, for example. Needless to say, the observation area of the crystal structure the observed grains can be selected as deemed appropriate or randomly.
  • each piezoelectric ceramic 11 layer (referring to the distance between an opposing pair of internal electrodes 12 , 13 ) is 10 ⁇ m or more but 60 ⁇ m or less. If the thickness of each piezoelectric ceramic 11 layer is less than 10 ⁇ m, the electric field intensity becomes too high for the voltage used, which is not desirable. If the thickness of each piezoelectric ceramic 11 layer exceeds 60 ⁇ m, on the other hand, the voltage to be used must be increased so as to increase the electric field intensity, which is not desirable, as a step-up circuit or other equipment becomes necessary.
  • FIG. 3 is a flow chart indicating the manufacturing method of piezoelectric element 10 pertaining to this embodiment. Each step is explained below. It should be noted that, in reality, each of the following steps can be carried out on one lot comprising many piezoelectric elements. In FIGS. 4 to 6 used in the explanation below, however, production of one piezoelectric element 10 at a time is assumed as a matter of convenience for illustration purposes.
  • material powders are weighed to achieve the target composition.
  • a material powder containing lithium lithium carbonate (Li 2 CO 3 ) can be used, for example.
  • a material powder containing sodium sodium carbonate (Na 2 CO 3 ) or sodium hydrogen carbonate (NaHCO 3 ) can be used, for example.
  • a material powder containing potassium potassium carbonate (K 2 CO 3 ) or potassium hydrogen carbonate (KHCO 3 ) can be used, for example.
  • a material powder containing niobium niobium pentoxide (Nb 2 O 5 ) can be used, for example.
  • tantalum tantalum pentoxide (Ta 2 O 5 ) can be used, for example.
  • the weighed material powders are mixed.
  • the material powders are sealed in a cylindrical pot, together with ethanol and partially stabilized zirconia (PSZ) balls, and mixed using the ball mill method.
  • PSZ partially stabilized zirconia
  • ethanol is evaporated and the remaining mixture is dried to obtain a mixed powder constituted by fully mixed material powders.
  • other organic solvent may be used instead of ethanol.
  • the mixed powder is calcined. Calcining is performed by holding the mixed powder in a crucible at a temperature of 700° C. to 950° C. for 1 hour to 10 hours. Then, the calcined compact is crushed using the ball mill method to obtain a calcined powder.
  • the material powder of the element which will constitute a sub phase as mentioned above is mixed into the calcined powder as necessary.
  • the ball mill method can also be used for this mixing.
  • manganese carbonate (MnCO 3 ), manganese monoxide (MnO), manganese dioxide (MnO 2 ), trimanganese tetraoxide (Mn 3 O 4 ), or manganese acetate (Mn(OCOCH 3 ) 2 ) can be used, for example.
  • manganese carbonate (MnCO 3 ), manganese monoxide (MnO), manganese dioxide (MnO 2 ), trimanganese tetraoxide (Mn 3 O 4 ), or manganese acetate (Mn(OCOCH 3 ) 2 ) can be used, for example.
  • NiO nickel monoxide
  • silicon dioxide (SiO 2 ) silicon dioxide (SiO 2 ) can be used, for example.
  • CaCO 3 calcium carbonate
  • BaCO 3 barium carbonate
  • strontium carbonate strontium carbonate
  • ZrO 2 zirconium oxide
  • the material powder need not contain only one type of element which will become a sub phase, but it may contain two or more types of elements which will become sub phases.
  • a material powder containing lithium and silicon lithium silicate (Li 2 SiO 3 ) or lithium orthosilicate (Li 4 SiO 4 ) can be used, for example.
  • a material powder containing calcium and silicon calcium metasilicate (CaSiO 3 ) or calcium orthosilicate (Ca 2 SiO 4 ) can be used.
  • calcium zirconium calcium zirconate (CaZrO 3 ) can be used.
  • strontium and zirconium strontium zirconate (SrZrO 3 ) can be used.
  • organic binder, dispersant, and pure water are added to the calcined powder and wet-mixed using the ball mil method to produce a ceramic slurry.
  • the ceramic slurry is formed into a sheet shape using the doctor blade method to obtain a ceramic sheet.
  • ethanol or other organic solvent may be used instead of pure water.
  • the thickness of the ceramic sheet can be controlled by the height of the blade on the doctor blade system and determined as deemed appropriate according to the structure of the piezoelectric element 10 .
  • the thickness of the ceramic sheet may be 20 ⁇ m, for example.
  • the manganese dispersion step is performed to form a manganese-rich phase 11 b , as shown in FIG. 2B on the ceramic sheet obtained in the aforementioned step (S1).
  • FIGS. 4A and 4B are schematic perspective views of the manganese dispersion step.
  • FIG. 4A is a view from the top side in the Z-axis direction
  • FIG. 4B is a view from the bottom side in the Z-axis direction.
  • a manganese dispersion layer 111 b in which manganese is uniformly dispersed is formed on both sides, in the Z-axis direction, of a ceramic sheet 111 a produced in the ceramic sheet production step, to produce a complex ceramic sheet 111 .
  • the manganese dispersion layer 111 b is constituted, for example, as a piezoelectric ceramic slurry whose composition contains more manganese-containing oxide than the ceramic sheet 111 a does.
  • the manganese dispersion layers 111 b are patterned according to the shapes of internal electrodes 12 , 13 shown in FIG. 2B .
  • the manganese dispersion layers 111 b can be formed by, for example, screen-printing the prepared slurry onto the ceramic sheet 111 a using screens on which the same patterns as the internal electrodes 12 , 13 are formed.
  • the manganese-rich phase 11 b is arranged in the entire area of the ceramic sheet 111 a , except for its outer peripheries, and has a projection that connects to one end in the Y-axis direction.
  • the projections on the top face and bottom face of the ceramic sheet 111 a in the Z-axis direction are formed in such a way that they face the opposite sides in the Y-axis direction, respectively.
  • the manganese-rich phase 11 b preferably covers the entire surfaces of the internal electrodes 12 , 13 in FIG. 2B , desirably the screens to be used for the manganese dispersion layer 111 b have patterns formed on them which are slightly larger than the patterns of internal electrodes 12 , 13 .
  • the manganese dispersion layers 111 b as manganese-rich phases 11 b adjacent to the internal electrodes 12 , 13 , which means that they can be formed over the entire surfaces on both sides of the ceramic sheet 111 a .
  • the manganese dispersion layers 111 b can be formed in a sheet shape using the doctor blade method separately from the ceramic sheet 111 a . Then, the sheet-shaped manganese dispersion layers 111 b are overlaid on both sides of the ceramic sheet 111 a.
  • the complex ceramic sheet 111 only needs to have manganese dispersed on both sides in the Z-axis direction, and need not constitute a layer like the manganese dispersion layer 111 b shown in FIG. 4 .
  • the complex ceramic sheet 111 may be a ceramic sheet 111 a having a manganese-containing oxide powder uniformly dispersed on both sides in the Z-axis direction.
  • a MnO fine powder can be dispersed using a sieve, for example, on both sides of the ceramic sheet 111 a in the Z-axis direction.
  • the internal electrode application step is performed to form internal electrodes 12 , 13 , as shown in FIG. 2B , on the complex ceramic sheet 111 obtained in the aforementioned step (S2).
  • FIGS. 5A and 5B are schematic perspective views of the internal electrode application step.
  • FIG. 5A is a view from the top side in the Z-axis direction
  • FIG. 5B is a view from the bottom side in the Z-axis direction.
  • a conductive paste (electrode paste) is applied to the top face, in the Z-axis direction, of the complex ceramic sheet 111 produced in the manganese dispersion step, to form an internal electrode film 112 .
  • the internal electrode film 112 is formed by screen-printing using a screen having internal electrode patterns formed on it.
  • the internal electrode film 112 is arranged in an area on the manganese dispersion layer 111 b .
  • the internal electrode film 112 is arranged in the entire area of the ceramic sheet 111 a , except for its outer peripheries, and has a projection 112 a that connects to one end in the Y-axis direction. These projections 112 a are where the internal electrodes 12 , 13 are connected to the external electrodes 14 , 15 .
  • the projection 112 a on the ceramic sheet 111 a is formed in such a way that its width is smaller than the part of ceramic sheet 111 a corresponding to the area where the internal electrodes 12 , 13 face each other.
  • the internal electrodes 12 , 13 shown in FIG. 2B are Pt electrodes
  • a conductive paste containing Pt was used for the internal electrode film 112 .
  • the conductive paste can be changed, as deemed necessary, according to the material of internal electrodes 12 , 13 .
  • Examples of internal electrodes 12 , 13 other than Pt electrodes include Pd electrodes and Ag—Pd electrodes.
  • the internal electrode film 112 is formed using a conductive paste containing Pd and conductive paste containing Ag and Pd, respectively.
  • an internal electrode film 112 was formed as shown in FIG. 5A after manganese dispersion layers 111 b were formed on both sides of the ceramic sheet 111 a as shown in FIGS. 4A and 4B .
  • a manganese dispersion layer 111 b may be formed only on the top face of the ceramic sheet 111 a in the Z-axis direction.
  • an internal electrode film 112 can be formed on the top face, in the Z-axis direction, of the manganese dispersion layer 111 b formed on the top face of the ceramic sheet 111 a in the Z-axis direction, after which a manganese dispersion layer 111 b may be formed on the top face of this internal electrode film 112 in the Z-axis direction.
  • FIG. 6 is a schematic perspective view of the ceramic sheet lamination step.
  • complex ceramic sheets 111 having the internal electrode film 112 obtained in the aforementioned step (S3) are laminated by a specified number of layers in such a way that their projections 112 a alternately face the opposite sides in the Y-axis direction.
  • the projections 112 a of the internal electrode films 112 on the laminated ceramic sheets 111 change their direction alternately by 180° around the Z-axis.
  • the laminate of complex ceramic sheets 111 is pressurized in the Z-axis direction, which is the laminating direction, to pressure-bond the layers into one piece.
  • the pressure applied to the laminate of complex ceramic sheets 111 in the Z-axis direction can be determined as deemed appropriate, such as 50 MPa.
  • a ceramic sheet 111 c 1 constituting the top layer in the Z-axis direction has neither manganese dispersion layer 111 b nor internal electrode film 112 formed on it, because there is no need to form an internal electrode film 112 on it.
  • a ceramic sheet 111 c 2 constituting the bottom layer in the Z-axis direction it is sufficient for a ceramic sheet 111 c 2 constituting the bottom layer in the Z-axis direction to have a manganese dispersion layer 111 b formed only on its top face in the Z-axis direction, because there is no internal electrode film 112 facing its bottom face.
  • the one-piece laminate obtained in the aforementioned step (S4) is sintered.
  • the laminate is stored in an alumina sheath and heated to a temperature of approx. 300° C. to 500° C. to remove the binder, followed by sintering in an atmosphere at a temperature of 900° C. to 1050° C. This way a sintered compact of laminate (ceramic sintered compact) is obtained.
  • external electrodes 14 , 15 as shown in FIGS. 2A and 2B are formed on the ceramic sintered compact obtained in the aforementioned step (S5).
  • FIGS. 7A and 7B are schematic perspective views of the external electrode forming step. As shown in the top figures of FIGS. 7A and 7B , ends of internal electrodes 12 , 13 formed from the aforementioned projections 112 a of internal electrode films 112 are exposed in a straight line, in the Z-axis direction, on both side faces of the ceramic sintered compact 100 in the Y-axis direction. In the external electrode forming step, external electrodes 14 , 15 are formed on both side faces of the ceramic sintered compact 100 in the Y-axis direction. The external electrode 14 covers one side of the ceramic sintered compact and connects all of the internal electrodes 12 . The external electrode 15 covers one side of the ceramic sintered compact and connects all of the internal electrodes 13 .
  • a conductive paste containing Ag, etc. is applied to both sides of the ceramic sintered compact 100 in the Y-axis direction, and baked at a temperature of approx. 750° C. to 850° C. This way, external electrodes 14 , 15 are formed as Ag electrodes on both sides of the ceramic sintered compact 100 in the Y-axis direction.
  • the piezoelectric element 10 is now complete.
  • external electrodes 14 , 15 need not be formed on the ceramic sintered compact 100 by means of baking. External electrodes 14 , 15 may be formed using the sputtering method, vacuum deposition method, or any other thin-film forming method, for example, as long as the formed electrodes can connect the internal electrodes 12 , 13 , respectively, in a favorable manner.
  • the piezoelectric ceramic 11 in the piezoelectric element 10 completed in the aforementioned step (S6) is polarized so as to make the piezoelectric element 10 usable as a piezoelectric actuator, etc.
  • Polarization is implemented by applying a high electric field between the external electrodes 14 , 15 of the piezoelectric element 10 .
  • the piezoelectric element 10 is put in silicone oil of 100° C. and an electric field of 3.0 kV/mm is applied for 15 minutes between the external electrodes 14 , 15 .
  • piezoelectric ceramic 11 shown in FIGS. 2A and 2B piezoelectric ceramics in which the mol number of manganese Mn was adjusted to 0, 0.2, 0.3 and 0.4 relative to 100 mol of the main phase expressed by Composition Formula (1) were produced.
  • the bright lines running in parallel at an equal pitch in each image represent the internal electrodes 12 , 13 , while bright points represent where manganese is present.
  • FIGS. 8B to 8D on the other hand, manganese is unevenly distributed near the internal electrodes 12 , 13 . Also from FIGS. 8B to 8D , manganese is uniformly distributed in the direction along the internal electrodes 12 , 13 . This trend is confirmed at Mn ⁇ 2.0.
  • the DC insulation longevity represents the relative time needed to achieve a current of 1 ⁇ A/cm 2 or more in current density after the start of application of a high DC electric field of 8 kV/mm between the external electrodes 14 , 15 of the piezoelectric element at 100° C.
  • the DC insulation longevity tended to increase as the content of Mn increased.
  • the AC insulation longevity was evaluated by driving the piezoelectric element 10 with a high AC electric field of 8 kV/mm, 100 Hz applied between the external electrodes 14 , 15 of the piezoelectric element 10 at 100° C.
  • the AC insulation longevity represents the relative number of times the piezoelectric element 10 is driven until it becomes no longer drivable.
  • Measurement of AC insulation longevity used an oscillator, voltage amplifier, and oscilloscope.
  • the AC insulation longevity tended to increase as the content of Mn increased.
  • the main phase of the piezoelectric ceramics is an alkali-containing niobate perovskite structure, but the main phase of the piezoelectric ceramics may represent other piezoelectric composition having excellent piezoelectric characteristics.
  • Examples of such piezoelectric composition include oxides of barium titanate perovskite structure and oxides of tungsten bronze structure.
  • the main phase of the piezoelectric ceramic is an alkali-containing niobate perovskite structure, but the main phase of the piezoelectric ceramic may represent other piezoelectric compositions having excellent piezoelectric characteristics.
  • piezoelectric compositions include oxides of barium titanate perovskite structure and oxides of tungsten bronze structure.
  • a piezoelectric element comprising first internal electrodes and second electrodes, as well as piezoelectric ceramic layers that are made of ceramics and arranged between the first internal electrodes and second internal electrodes, wherein manganese is present relatively more abundantly in areas of the piezoelectric ceramic layers adjacent to the first internal electrodes and second internal electrodes, compared to at centers of the piezoelectric ceramic layers.
  • a piezoelectric element according to any one of 1) to 7), further comprising a first external electrode and second external electrode, wherein the first internal electrodes and second internal electrodes are alternately arranged via the piezoelectric ceramic layers, and the first internal electrodes are each connected to the first external electrode and the second internal electrodes are each connected to the second external electrode.
  • a piezoelectric element according to 10 wherein the main phase is expressed by a composition formula (Li x Na y K 1-x-y ) a (Nb 1-z Ta z )O 3 (in the formula, 0.04 ⁇ x ⁇ 0.1, 0 ⁇ y ⁇ 1, 0 ⁇ z ⁇ 0.4, 0.95 ⁇ a ⁇ 1.01, and x+y ⁇ 1).
  • piezoelectric element according to 10) or 11), wherein the piezoelectric ceramic layers contain manganese at a ratio of 0.2 mol or more but 2.0 mol or less relative to 100 mol of the main phase.
  • a manufacturing method of piezoelectric element comprising:
  • any ranges applied in some embodiments may include or exclude the lower and/or upper endpoints, and any values of variables indicated may refer to precise values or approximate values and include equivalents, and may refer to average, median, representative, majority, etc. in some embodiments.
  • an article “a” or “an” may refer to a species or a genus including multiple species, and “the invention” or “the present invention” may refer to at least one of the embodiments or aspects explicitly, necessarily, or inherently disclosed herein. In this disclosure, any defined meanings do not necessarily exclude ordinary and customary meanings in some embodiments.
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